CN109651851A - The inorganic-organic hybridization nano pigment and preparation method of natural botanical source and application - Google Patents

The inorganic-organic hybridization nano pigment and preparation method of natural botanical source and application Download PDF

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Publication number
CN109651851A
CN109651851A CN201910036575.1A CN201910036575A CN109651851A CN 109651851 A CN109651851 A CN 109651851A CN 201910036575 A CN201910036575 A CN 201910036575A CN 109651851 A CN109651851 A CN 109651851A
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pigment
natural
nano
inorganic particle
stabilizer
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周超
宋荣耀
袁赛萍
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Shanghai Chongming Mumianhuakai Hand Club
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Shanghai Chongming Mumianhuakai Hand Club
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/56Treatment of carbon black ; Purification
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25Silicon; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/737Galactomannans, e.g. guar; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/04Preparations containing skin colorants, e.g. pigments for lips
    • A61Q1/06Lipsticks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/08Preparations containing skin colorants, e.g. pigments for cheeks, e.g. rouge
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/3607Titanium dioxide
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08Treatment with low-molecular-weight non-polymer organic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

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Abstract

The invention discloses the inorganic-organic hybridization nano pigment and preparation method of a kind of natural botanical source and applications, for natural plant pigment, nano inorganic particle, stabilizer and coating material hybrid, the weight ratio of each component are as follows: natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.2~3:0.2~0.7:0.2~1.5.The present invention can be used for the fields such as cosmetics, food, drug, children's pigment, raw material sources of the present invention are abundant, it is safe and healthy, colour system is more complete, compared with synthetic dyestuff tone more naturally, having certain healthcare function, color is relatively bright-coloured, the majority organic reagent such as not soluble in water, ethyl alcohol, there is preferable dispersibility, photo and thermal stability, tinting strength, tinting power.Especially suitable for coated tablet, candy, the coloring of high-end cosmetics, it is also applied for the coloring of daily chemical products, hair dye, ink, rubber, toy for children, underwear product, is had a extensive future.

Description

The inorganic-organic hybridization nano pigment and preparation method of natural botanical source and application
Technical field
The present invention relates to a kind of natural plants pigment and its preparation method and application.
Background technique
Organic pigment has the advantages that wide color gamut, color clear, tinting strength, tinting power are outstanding, but compared with inorganic pigment, valence Lattice are expensive, and durability, in terms of there are problems.But in daily production and life, organic compared to inorganic pigment Pigment is more favored and favorable comment.Organic pigment is mainly used for coating, ink, rubber, fiber, paper processed, leather, cosmetics etc..But The organic pigment for being synthesis is all that chemical method obtains mostly, and raw material water solubility synthetic dyestuff is mostly with chemical industry such as benzene, toluene, naphthalenes Product is raw material, is formed by a series of organic reactions such as sulfonation, nitrification, azos, contains R-N, N-R ' key, phenyl ring mostly Or xanthene structural compounds, thus many synthetic organic pigments have certain toxicity, it is necessary to strict control using kind, range and Quantity limits acceptable daily intake (ADI).
Some organic pigment long-term low doses intake, there is also teratogenesis, it is carcinogenic a possibility that.Compared to the organic face of synthesis Material, natural plant dye is nontoxic, ecology, and color is soft, certainly however characteristic, and it has good Environmental compatibility and medicine Object health properties, thus be concerned, especially become the new lover of colorant in cosmetics, medicines and health protection, juvenile product field, There is vast potential for future development.
It is most of that dyestuff is extracted by heating by water or solvent from the point of view of the dyeing of current natural plant dye, And dye liquor is directly used in the dyeing of textile.The method has a disadvantage that 1. dye moiety is thermally decomposed, and stability is poor;② The sublimation characteristics of natural plant dye are destroyed;3. it is perishable, it should not store;4. reproducibility is difficult to grasp.To solve The above problem, 108795096 A natural plants color lake Chinese invention patent application publication number CN and preparation method thereof, middle promulgated by the State Council Preparation process, color lake and its application in bright 108864744 color lake A patent application publication number CN will be natural using color lake technology Vegetable colour makes its precipitating become natural plants color lake by metallic compound precipitator, improves the stability of vegetable colour with it, protects Matter phase and reproducibility.But this method just with the complexing of metal ion be dye molecule combine formed it is big insoluble Property particle, structure is still unstable, and granular size is unable to control during forming particle, the particle generally formed All larger, this brings difficulty to subsequent coloring application.Appoint at present and so lacks a kind of stable, size tunable, coloring energy The strong natural plants pigment of power and its preparation method.
Summary of the invention
The purpose of the present invention is disclose a kind of inorganic-organic hybridization nano pigment of natural botanical source and preparation method and answer With to overcome the defect of the above-mentioned prior art.
The inorganic-organic hybridization nano pigment of the natural botanical source is natural plant pigment, nano inorganic The hybrid of grain, stabilizer and coating material, the weight ratio of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material
=1:0.2~3:0.2~0.7:0.2~1.5;
Preferably, the weight percent of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material
=1:0.4~2.5:0.3~0.65:0.3~1.2;
The natural plants include blue mountain, wood indigo plant, woaded blue, indigo plant, moon tangerine, marigold, turmeric, water cape jasmine, good fortune wood, Chinese scholartree One of tree, bush, Chinese tallow tree, Chinese gall, pomegranate, walnut, madder, strike, safflower, wormwood, tea tree, red yeast rice, Asian puccoon etc. with On;
The nano inorganic particle is white carbon black, mesoporous silicon oxide, P25 (titanium dioxide), mesoporous TiO 2, oxygen Change one or more of cerium, zirconium oxide, magnesia, aluminium oxide etc., partial size is 10~500 nanometers;
The stabilizer be F127, Span, tween, P123, gelatin, gum arabic powder, melon rubber powder, chitosan, Its more than one such as agar powder;
Wherein, the chemical name of F127 is poly- (the propylene glycol)-poly(ethylene glycol) triblock copolymer of poly(ethylene glycol)-, can Use the Sigma company trade mark for the product of P2443, the chemical name of P123 is polyethylene oxide-polypropylene oxide-polycyclic oxygen second The product that the Sigma company trade mark is 106392-12-5 can be used in alkane triblock copolymer;
The surface modification is alum, calcium sulfate, calcium oxalate, calcium acetate, calcium chloride, aluminium chloride, aluminum sulfate, Ta Ta Powder, aluminum acetate, one or more of ferric acetate etc.;
The inorganic-organic hybridization nano pigment of the natural botanical source obtains preparation method, comprising the following steps:
(1) natural plants dyeing liquor is mixed with nano inorganic particle dispersion, pH adjusting agent is added and adjusts pH=6-8, Precipitating obtains sediment;
The natural plants dyeing liquor is the mixture containing natural plant pigment and solvent;
The nano inorganic particle dispersion is nano inorganic particle, stabilizer, coating material and aqueous mixtures;
The weight ratio of nano inorganic particle, stabilizer and coating material are as follows:
Nano inorganic particle, stabilizer and coating material=0.2~3:0.2~0.7:0.2~1.5;
Preferably 0.4~2.5:0.3~0.65:0.3~1.2;
Solid-liquid ratio is 1:3-30, and solid-liquid ratio is nano inorganic particle, the total weight of stabilizer and coating material and water Weight ratio g/mL;
The solvent be water or be volumetric concentration 50%-90% ethyl alcohol;
The pH adjusting agent is hydrochloric acid or sodium hydroxide;
The volumetric usage of natural plants dyeing liquor and the nano inorganic particle dispersion in step (2), is contaminated with natural plants Nano inorganic particle, stabilizer and surface in color liquid in the nano inorganic particle dispersion of the weight sum of natural plant pigment are repaired It adorns on the basis of the weight of agent, are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material
=1:0.2~3:0.2~0.7:0.2~1.5;
Preferably, the weight percent of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.4~2.5:0.3~0.65:0.3 ~1.2;
In natural plants dyeing liquor, the weight of the natural plant pigment can be using conventional weighing drying means It determines;
Preferably, one of the preparation method of the natural plants dyeing liquor, includes the following steps:
Natural plant pigment is mixed with solvent, obtains the solution containing natural plant pigment, as natural plants dye Liquid, the natural plant pigment can be used commercially produced product or use " Study on extraction of total saponin of sapindusmukerossi, Anhui Agricultural sciences, Journal of Anhui Agri.Sci.2010,38 (1): 354-356. " method preparation reported in the literature;
Preferably, the two of the preparation method of the natural plants dyeing liquor, include the following steps:
By pigment composition of the natural plants in extraction natural plants, filtering obtains natural plants dyeing liquor;
Preferably, first natural plants are crushed, sieving, then pulverizes and sieves to obtain 200 mesh powder below, then with damp and hot Steam treatment 1~3 hour, then with the pigment in extraction natural plants, thick natural plants dyeing liquor is obtained, is stirred molten Solution, filtering, as the natural plants dyeing liquor;
The solvent be water or be volumetric concentration 50%-90% ethyl alcohol;
Solid-liquid ratio is 1:3-30, and solid-liquid ratio is the ratio between weight and the solvent volume of natural plants g/mL;
Extraction time is 30min-360min, and extraction temperature is 30-75 DEG C;
(2) then from the sediment, the inorganic-organic hybridization nano face of the day natural botanical source is collected Material;
Preferably, the collection method, being separated by filtration including sediment, washing, -40~-45 DEG C of freeze-dryings 20 ~28h.
The inorganic-organic hybridization nano pigment of natural botanical source of the present invention derives from natural plants to be a kind of Pigment, can be used for the fields such as cosmetics, food, drug, children's pigment, application method and conventional dyestuff such as gouache color, Colorant additive, color lake etc. are identical, such as 108864744 A of CN method reported in the literature.
The invention has the benefit that the raw material that (1) present invention uses is mountain indigo plant, wooden indigo plant, woaded blue, indigo plant, moon tangerine, Wan Shou Chrysanthemum, turmeric, water cape jasmine, good fortune wood, Chinese scholartree, bush, Chinese tallow tree, Chinese gall, pomegranate, walnut, madder, strike, safflower, wormwood, tea The natural plants such as tree, red yeast rice, Asian puccoon, raw material sources are abundant, and safe and healthy, colour system is more complete, more certainly compared with synthetic dyestuff tone So, and pigment extract contains multiple efficacies ingredient, has certain healthcare function, can satisfy people to safety, natural, more The requirement of function.(2) stabilizer uses amphipathy macromolecule, Nantural non-toxic.(3) coating material uses metal salt starting materials, no Containing heavy metal, safe and non-toxic, simple process, Product Safety is high.(4) this method is simple, be multicolour, multi-functional, high stable, High adhesion force vegetable pigment provides new thinking.(5) pigment be water-soluble organic pigment is precipitated, moditied processing preparation Made of, compared with its water colo(u)r, color is relatively bright-coloured, and the majority organic reagent such as not soluble in water, ethyl alcohol has preferable dispersion Property, photo and thermal stability, tinting strength, tinting power.Especially suitable for coated tablet, candy, high-end cosmetics coloring, be also applied for daily chemical products, The coloring of hair dye, ink, rubber, toy for children, underwear product, has a extensive future.
Detailed description of the invention
Fig. 1 is the inorganic-organic hybridization nano pigment schematic diagram of the natural botanical source of natural botanical source.
Fig. 2 is the photo in kind of embodiment 1.
Fig. 3 is the inorganic-organic hybridization nano pigment electron microscope of the natural botanical source of embodiment 1.
Specific embodiment
Below with reference to the embodiment of the present invention, the invention will be further elaborated.
Referring to Fig. 1, the inorganic-organic hybridization nano pigment of the natural botanical source for natural plant pigment 1, is received The hybrid of rice inorganic particle 2, stabilizer 3 and coating material 4.
Embodiment 1
The inorganic-organic hybridization nano pigment of wooden indigo plant (blue) natural botanical source
The weight ratio of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:2.5:0.375:1.125;
Wherein:
Natural plant pigment is the wooden cyanine, and nano inorganic particle is white carbon black, and partial size is 100 nanometers, and stabilizer is P123, coating material are alum;
Preparation method:
(1) natural plants dyeing liquor is prepared: the wooden blue powder is broken, sieving, then pulverize and sieve to obtain 200 mesh powder below, Then 2h is handled with wet-hot steam, with the pigment in the alcohol steep natural plants of volume 60%, can be obtained described natural Plant dyeing liquid;
Solid-liquid ratio is 1:5, and extraction time 60min, extraction temperature is 35 DEG C;Mixing speed is 800rpm;
(2) it prepares nano inorganic particle dispersion: nano inorganic particle white carbon black, stabilizer and surface being added in water and repairs Agent is adornd, nano inorganic particle dispersion is obtained;
In the nano inorganic particle dispersion, titanium dioxide, stabilizer and coating material weight ratio are as follows: 2.5: 0.375:1.125, solid-liquid ratio 1:3g/mL;
(3) hybrid inorganic-organic: the nanoparticle in natural plants dyeing liquor and step (2) that step (1) is obtained point Dispersion liquid mixing, then the speed of 1000rpm stirs 0.5h, adjusts pH=6 with HCl, continues to stir 1h, finally stands overnight nature Precipitating;
The volumetric usage of natural plants dyeing liquor and the nano inorganic particle dispersion in step (2), is contaminated with natural plants Nano inorganic particle, stabilizer and surface in color liquid in the nano inorganic particle dispersion of the weight sum of natural plant pigment are repaired It adorns on the basis of the weight of agent, are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:2.5:0.375:1.125;(weight Than);
(4) pigment separates: the sediment that step (3) obtains is centrifuged, centrifugal speed 3000rpm/min, Obtain sediment;
(5) wash: the precipitating that step (4) is obtained is with water washing 3 times of 10 times, and then -45 DEG C of dryings for 24 hours, can obtain Obtain the inorganic-organic hybridization nano pigment of the natural botanical source.Electromicroscopic photograph such as Fig. 1.Photo in kind is shown in Fig. 2
Wooden indigo plant-nano dye of acquisition is used for children's pigment, application method is as follows:
(1) powdered wooden indigo plant-nano dye is weighed by preset weight ratio, is then added into the bottom of children's pigment In object;
(2) decentralized processing is carried out to mixture with high speed disperser, obtains uniform and stable colored pigment;
(3) product is packed, obtains product.
It is detected using EN71-3 standard, as a result as follows:
Sb (antimony) (< 60ppm), As (arsenic) (< 25ppm), Ba (barium) (< 1000ppm), Cd (cadmium) (< 75ppm), Cr (chromium) (< 60ppm), Pb (lead) (< 90ppm), Hg (mercury) (< 60ppm), Se (selenium) (< 500ppm).
Embodiment 2
The weight ratio of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:1:0.375:0.5
Natural plant pigment is curcumin, and nano inorganic particle is that nanoparticle is titanium dioxide, and partial size is received for 200nm Rice, stabilizer is gum arabic powder, and coating material is calcium acetate;
The preparation method is as follows:
(1) it prepares natural plants dyeing liquor: turmeric being crushed, sieving, then pulverize and sieve to obtain 200 mesh powder below, Then 2h is handled with wet-hot steam, finally with the pigment in 70% alcohol steep natural plants, solid-liquid ratio 1:10g/mL, leaching Mentioning the time is 120min, and extraction temperature is 50 DEG C;Mixing speed is 800rpm;
(2) it prepares nano inorganic particle dispersion: titanium dioxide, stabilizer and coating material being added in water, obtain Nano inorganic particle dispersion;
In the nano inorganic particle dispersion, the weight ratio of titanium dioxide, stabilizer and coating material are as follows: 1: 0.375:0.5;Solid-liquid ratio is 1:30g/mL;
(3) hybrid inorganic-organic: the nano inorganic in natural plants dyeing liquor and step (2) that step (1) is obtained Grain dispersion liquid mixing, then the speed of 800rpm stirs 0.5h, adjusts pH=8 with NaOH, continues to stir 1.5h, finally stand Night natural sedimentation;
The volumetric usage of natural plants dyeing liquor and the nano inorganic particle dispersion in step (2), is contaminated with natural plants Nano inorganic particle, stabilizer and surface in color liquid in the nano inorganic particle dispersion of the weight sum of natural plant pigment are repaired It adorns on the basis of the weight of agent, are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.375:0.5;
(4) pigment separates: the sediment that step (3) obtains is centrifuged, centrifugal speed 3000rpm/min, Obtain sediment.
(5) wash: the precipitating that step (4) is obtained is with water washing 2 times of 10 times, by -40 DEG C of sediment dry 28h, i.e., The inorganic-organic hybridization nano pigment of the natural botanical source can be obtained.
The pigment of acquisition is used to colour hand cleanser and dish washing detergent, application method is as follows:
(1) powdered turmeric-nano dye is weighed by preset weight ratio, is then added into hand cleanser or washing In the substrate of agent;
(2) decentralized processing is carried out to mixture with high speed disperser, obtains uniform and stable coloured hand cleanser and tableware and washes Wash agent;
(3) product is packed, obtains product.
It is detected using GB/T 5211.6-1985 standard, as a result as follows:
The acid resistance of pigment with the staining of filtrate than rank, the discoloration rank of filter cake or simultaneously with the staining rank of filtrate and The discoloration rank of filter cake indicates.Filtrate staining, preferably 5 grades of filter cake discoloration, worst is 1 grade.Filtrate staining degree is between It is indicated with 4~5,3~4,2~3,1~2.The discoloration of filter cake is used 4/5,3/4,2/3,1/2 indicate between.As simultaneously When expression filtrate staining degree and the rank of filter cake discoloration, then it represents that be A [B] that A indicates filtrate staining rank, [B] filter cake Change colour rank.
Test result shows that the acid resistance rank of pigment is 4~5 [5].
Embodiment 3
The weight ratio of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.4:0.3:0.3;
Natural plant pigment is carthamin, and nano inorganic particle is the mixture of white carbon black and titanium dioxide, weight ratio For 1:1, partial size is 300nm nanometers, and stabilizer is melon rubber powder, and coating material is tower tower powder;
Preparation method:
(1) it prepares natural plants dyeing liquor: safflower being crushed, sieving, then pulverize and sieve to obtain 200 mesh powder below, Then 2h is handled with wet-hot steam, finally with the pigment composition in 80% alcohol steep natural plants, solid-liquid ratio 1:30, material Liquor ratio is that unit is g/mL, and extraction time 360min, extraction temperature is 65 DEG C;Mixing speed is 1200rpm.
(2) it prepares nano inorganic particle dispersion: nano inorganic particle, stabilizer and coating material being added in water, Obtain nano inorganic particle dispersion;
In the nano inorganic particle dispersion, the weight ratio of nano inorganic particle, stabilizer and coating material are as follows: 0.4:0.3:0.3;Solid-liquid ratio is 1:30g/mL;
(3) hybrid inorganic-organic: the nanoparticle in natural plants dyeing liquor and step (2) that step (1) is obtained point Dispersion liquid mixing, then the speed of 1200rpm stirs 0.5h, adjusts pH=7 with HCl, continues to stir 2h, finally stands overnight nature Precipitating,
The volumetric usage of natural plants dyeing liquor and the nano inorganic particle dispersion in step (2), is contaminated with natural plants Nano inorganic particle, stabilizer and surface in color liquid in the nano inorganic particle dispersion of the weight sum of natural plant pigment are repaired It adorns on the basis of the weight of agent, are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.4:0.3:0.3;
(4) pigment separates: the sediment that step (3) obtains is centrifuged, centrifugal speed 3000rpm/min, Obtain sediment;
(5) wash: by step (4) obtain precipitating with 10 times of water carry out wash 3 times, then -45 DEG C of dryings for 24 hours, i.e., It can get the inorganic-organic hybridization nano pigment of the natural botanical source.
The pigment of acquisition is used for colored cosmetic, application method is as follows:
(1) powdered safflower-nano dye is weighed by preset weight ratio, is then added into cosmetics (espespecially Kermes, lipstick) substrate in;
(2) decentralized processing is carried out to mixture with high speed disperser, obtains uniform and stable kermes, lipstick;
(3) product is packed, obtains product.
It is detected using GB/T9735-2008 standard, as a result as follows:
Pb (lead) (< 80ppm), Hg (mercury) (< 50ppm), Se (selenium) (< 800ppm).

Claims (11)

1. the inorganic-organic hybridization nano pigment of natural botanical source, which is characterized in that be natural plant pigment, nano inorganic The hybrid of particle, stabilizer and coating material, the weight ratio of each component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.2~3:0.2~0.7:0.2~1.5.
2. the inorganic-organic hybridization nano pigment of natural botanical source according to claim 1, which is characterized in that each The weight percent of component are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.4~2.5:0.3~0.65:0.3~ 1.2。
3. the inorganic-organic hybridization nano pigment of natural botanical source according to claim 1 or 2, which is characterized in that institute The natural plants stated include mountain indigo plant, wooden indigo plant, woaded blue, indigo plant, moon tangerine, marigold, turmeric, water cape jasmine, good fortune wood, Chinese scholartree, bush, crow One or more of Chinese tallow tree, Chinese gall, pomegranate, walnut, madder, strike, safflower, wormwood, tea tree, red yeast rice, Asian puccoon.
4. the inorganic-organic hybridization nano pigment of natural botanical source according to claim 1 or 2, which is characterized in that institute The nano inorganic particle stated is white carbon black, mesoporous silicon oxide, P25 (titanium dioxide), mesoporous TiO 2, cerium oxide, oxidation One or more of zirconium, magnesia, aluminium oxide.
5. the inorganic-organic hybridization nano pigment of natural botanical source according to claim 1 or 2, which is characterized in that institute The stabilizer stated be F127, Span, tween, P123, gelatin, gum arabic powder, melon rubber powder, chitosan, agar powder its More than one.
6. the inorganic-organic hybridization nano pigment of natural botanical source according to claim 1 or 2, which is characterized in that institute The surface modification stated is alum, calcium sulfate, calcium oxalate, calcium acetate, calcium chloride, aluminium chloride, aluminum sulfate, tower tower powder, aluminum acetate, vinegar One or more of sour iron.
7. the preparation side of the inorganic-organic hybridization nano pigment of described in any item natural botanical sources according to claim 1~6 Method, which comprises the following steps:
(1) natural plants dyeing liquor is mixed with nano inorganic particle dispersion, pH adjusting agent is added and adjusts pH=6-8, precipitates, Obtain sediment;
The natural plants dyeing liquor is the mixture containing natural plant pigment and solvent;
The nano inorganic particle dispersion is nano inorganic particle, stabilizer, coating material and aqueous mixtures;
(2) then from the sediment, the inorganic-organic hybridization nano pigment of the natural botanical source is collected.
8. the method according to the description of claim 7 is characterized in that the collection method, being separated by filtration including sediment, Washing, -40~-45 DEG C of 20~28h of freeze-drying.
9. the method according to the description of claim 7 is characterized in that the weight of nano inorganic particle, stabilizer and coating material Measure ratio are as follows: nano inorganic particle, stabilizer and coating material=0.2~3:0.2~0.7:0.2~1.5;
The volumetric usage of natural plants dyeing liquor and the nano inorganic particle dispersion in step (2), with natural plants dyeing liquor Nano inorganic particle, stabilizer and coating material in the nano inorganic particle dispersion of the weight sum of middle natural plant pigment Weight on the basis of, are as follows:
Natural plant pigment: nano inorganic particle: stabilizer: coating material=1:0.2~3:0.2~0.7:0.2~1.5.
10. the method according to the description of claim 7 is characterized in that the preparation method of the natural plants dyeing liquor, including Following steps:
Natural plant pigment is mixed with solvent, obtains the solution containing natural plant pigment, as natural plants dyeing liquor, or Person:
By pigment composition of the natural plants in extraction natural plants, filtering obtains natural plants dyeing liquor;Or:
First natural plants are crushed, sieving, then pulverize and sieve to obtain 200 mesh powder below, then with wet-hot steam processing 1~ 3 hours, then with the pigment in extraction natural plants, thick natural plants dyeing liquor is obtained, stirring and dissolving filters, as The natural plants dyeing liquor;
The solvent be water or be volumetric concentration 50%-90% ethyl alcohol;
Solid-liquid ratio is 1:3-30, and solid-liquid ratio is the ratio between weight and the solvent volume of natural plants g/mL;
Extraction time is 30min-360min, and extraction temperature is 30-75 DEG C.
11. the application of the inorganic-organic hybridization nano pigment of described in any item natural botanical sources according to claim 1~6, It is characterized in that, being used for cosmetic pigment, food pigment, drug pigment or children's pigment.
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CN113402900A (en) * 2021-06-15 2021-09-17 北京工商大学 Composite pigment of natural mesoporous mineral and animal and plant pigment and preparation method thereof
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